KR100661972B1 - Method for producing coated member of nanolayer and coated member of nanolayer - Google Patents

Abstract

The cutting tool 20 coated with a nanolayer has a substrate 30 and the substrate has surfaces 38, 40 with a coating 32 on its surface. The coating has a plurality of coating sets of alternating nanolayers of metal aluminum nitride and metal nitride and / or metal aluminum carbon nitride, each coating set having a thickness of up to about 100 nanometers. The coating has a bonding region 34 and an outer region 36. Bonding region 34 has a plurality of coating sets, the thickness of each coating set increases as one of them is located farther from the surface of the substrate. The outer region 36 has a plurality of coating sets, with each coating set being approximately equal in thickness.

Description

Nanolayered coated member and process for making a nanolayered coated member}

The present invention relates to a cutting tool coated with multiple layers and a method of manufacturing the same. More specifically, the present invention relates to a nanolayered coated cutting tool and a method of making the same. In this regard, a cutting tool coated with a nanolayer has a coating scheme having adjacent coated nanolayers having a thickness of about 100 nanometers or less.

Cutting tools coated with nanolayers exhibit excellent metal cutting properties in certain environments. Typically, a coating cutting tool consisting of multiple layers has a substrate having a plurality of coating layers deposited thereon. In some examples the coating layers have a plurality of alternating coating layers. In this regard, US Pat. No. 6,103,357 to Cylinder et al., For cutting tools coated with multiple layers, discloses a structure of non-repetitive coatings in which the layers have a thickness ranging from 0.1 to 30 nanometers. Initiate. PCT patent application WO 98/44163, filed by Sjostrand et al. For cutting tools coated with multiple layers, has a multi-layer repeated coating having a thickness in which each repetition period is in the range between 3 and 100 nanometers. Initiate organization.

Other exemplary coating tissues include multilayer titanium nitride / titanium aluminum nitride coatings deposited by physical vapor deposition (PVD) technology. Such coating tissues are described by Hsieh's "TiAlN using Unbalanced Electron Sputtering and Multilayer TiN / TiAlN" (Surface and Coating Technology 108-109 (1998) pages 132-137), and by Anderson et al. "Deposition, Microstructure, and Mechanical and Friction Properties of Electron Tube Sputtered TiN / TiAlN Multilayers" (Surface and Coating Technology 123 (2000) pages 219-226).

Although there may be multiple layers of titanium nitride / titanium aluminum nitride coating tissues, the coating must have a certain minimum adhesion to the substrate and exhibit a certain minimum hardness to be effective. Improving the adhesion of the coating to the substrate of the coated cutting tool has always been a goal and still is. Moreover, optimizing the hardness of coated cutting tools has always been a goal and still is. Improving and optimizing the combination of hardness and adhesion properties of coated cutting tools has always been a goal and still is.

Thus, there is a need for providing a coated cutting tool (eg, a nanolayer coated cutting tool) as well as a method of manufacturing a coated cutting tool, where the cutting tool is improved in a combination of adhesion and hardness. As well as improved adhesion and optimized hardness.

It also requires the provision of a coated cutting tool of metal nitride / metal aluminum nitride (eg, a cutting tool coated with nanolayers of titanium nitride / titanium aluminum nitride) as well as a method of manufacturing coated cutting tools. The cutting tool here is not only an improvement in the combination of adhesion and hardness, but also an optimized hardness and improved adhesion.

There is also a need to provide not only methods of making coated cutting tools, but also cutting tools of metal aluminum nitride / metal aluminum carbon nitride coatings (e.g., titanium aluminum nitride / titanium aluminum carbon nitride coated cutting tools of nanolayers). Here, the cutting tool is not only improved in the combination of attachment and hardness, but also has improved adhesion and optimized hardness.

In addition to methods of making coated cutting tools, cutting tools coated with metal nitride / metal aluminum nitride / metal aluminum carbon nitride (e.g., coated with nano nitrides of titanium nitride / titanium aluminum nitride / metal aluminum carbon nitride) It is necessary to provide a cutting tool, which is not only improved in a combination of attachment and hardness, but also has improved adhesion and optimized hardness.

In one aspect, the invention is a coated member of a nanolayer comprising a substrate having a surface and a coating on the substrate surface. The coating comprises a coating set of a plurality of nanolayers, one set of nanolayers of metal nitrides (where the metal nitrides may optionally comprise carbon and / or silicon) and nanolayers of metal aluminum nitrides With alternating nanolayers of metal aluminum nitride, which may optionally comprise carbon and / or silicon. The coating has a bonding area and an outer area. The bonding area has a plurality of coating sets, the thickness of which is generally increased as one is located away from the surface of the substrate. The outer region has a plurality of coating sets. The metal may be a combination of titanium, niobium, hafnium, vanadium, tantalum, zirconium and / or chromium alone or in combination with each other, or as long as the composition of the metal nitride layer is different from that of the metal aluminum nitride layer. It may be provided in combination with other metals including.

In another aspect, the present invention is a coated member of a nanolayer comprising a substrate having a surface and a coating on the surface of the substrate. The coating has a coated set of a plurality of nanolayers, one set of which is a nanolayer of metal aluminum nitride, where the metal aluminum nitride may optionally comprise carbon and / or silicon, and metal aluminum carbon nitride With alternating nanolayers of nanolayers, wherein the metal aluminum carbon nitride optionally comprises silicon. The coating has a bonding area and an outer area. The bond area has a plurality of coating sets, the thickness of the coating set generally increasing as it is located far from the surface of the substrate. The outer region has a plurality of coating sets. The metal may be provided with titanium, niobium, hafnium, vanadium, tantalum, zirconium and / or chromium alone or in combination with each other, or in combination with other metals.

In another aspect, the invention is a coated member of a nanolayer having a substrate having a surface and a coating on the surface of the substrate. The coating comprises a coating set of a plurality of nanolayers, where one set is a nanolayer of metal nitride (where the metal nitride may optionally comprise carbon and / or silicon), a nanolayer of metal aluminum nitride (Where the metal aluminum nitride may optionally comprise carbon and / or silicon) and an alternating nanolayer of metal aluminum carbon nitride (where the metal aluminum carbon nitride may optionally comprise silicon). It is provided with nano layers. The coating has a bonding area and an outer area. The bonding area has a plurality of coating sets, the thickness of which increases overall as one of them is located farther from the substrate surface. The outer region has a plurality of coating sets. The metal may be titanium, niobium, hafnium, vanadium, tantalum, zirconium and / or chromium alone or in combination with each other, or the composition of the metal nitride layer is different from that of the metal aluminum nitride layer and the metal aluminum carbon nitride layer. The lower surface may be combined with other metals having aluminum in the metal nitride layer.

In another aspect, the invention provides a method of making a coated member of a nanolayer, the method comprising providing a substrate having a surface; Providing a metal target (the metal target may optionally have carbon and / or silicon); Providing a metal-aluminum target (the metal-aluminum target may optionally comprise carbon and / or silicon); Rotating the substrate between the metal target and the metal-aluminum target; Supplying a first level of power to the metal target; Depositing a coating having a coating set of alternating nanolayers on the surface of the substrate; Varying the deposition rate of alternating nanolayer thickness over a first period of time while the power supplied to the metal target is changing from the first level to the second level; And controlling the deposition rate of alternating nanolayer thicknesses during the second time period after the power reaches the second level. The metal comprises aluminum in the metal target alone, in combination with titanium, niobium, hafnium, vanadium, tantalum, zirconium and / or chromium, or as long as the composition of the metal target is different from that of the metal-aluminum target. It can be provided in combination with other metals.

In another aspect, the invention relates to a method of making a coated member of a nanolayer, the method comprising providing a substrate having a surface; Providing a metal-aluminum target (the metal-aluminum target may optionally comprise carbon and / or silicon); Providing a metal-aluminum-carbon target (the metal-aluminum-carbon target may optionally have silicon); Rotating the substrate between the metal-aluminum target and the metal-aluminum-carbon target; Supplying power to the metal-aluminum target at a first level; Supplying power to the metal-aluminum-carbon target at a first level; Depositing a coating having a coating set of alternating nanolayers on the surface of the substrate; Varying the deposition rate of alternating nanolayer thicknesses over a first time period while the power supplied to the metal-aluminum target and the metal-aluminum carbon target is changing from the first level to the second level; And controlling the deposition rate of alternating nanolayer thicknesses during the second time period after the power reaches the second level. The metal may be provided with titanium, niobium, hafnium, vanadium, tantalum, zirconium and / or chromium alone or in combination with each other, or in combination with other metals.

In another aspect, the invention relates to a method of making a coated member of a nanolayer, the method comprising: providing a substrate having a surface; Providing a metal target (the metal target may optionally comprise carbon and / or silicon); Providing a metal-aluminum target (the metal-aluminum target may optionally comprise carbon and / or silicon); Providing a metal-aluminum-carbon target (the metal-aluminum-carbon target may optionally comprise silicon); Rotating the substrate between the metal target and the metal-aluminum target and the metal-aluminum-carbon target; Supplying power to the metal target at a first level; Supplying power to the metal-aluminum target at a first level; Supplying power to the metal-aluminum-carbon target at a first level; Depositing a coating set having a coating set of alternating nanolayers on the surface of the substrate; Varying the deposition rate of alternating nanolayer thickness during a first time period during which power supplied to the metal target and the metal-aluminum target and the metal-aluminum-carbon target are changed from the first level to the second level; And controlling the deposition rate of alternating nanolayers thickness during the second time period after the power reaches the second level. The metal may be titanium, niobium, hafnium, vanadium, tantalum, zirconium and / or chromium alone or in combination with each other, or the composition of the metal target is different from that of the metal-aluminum target and the metal-aluminum-carbon target. If any, in combination with other metals including aluminum in the metal target.

The following is a brief description of the drawings forming part of this application.

1 is an illustration of an equal magnification for a particular embodiment of a cutting tool coated with a nanolayer.

FIG. 2 is a schematic cross-sectional view of the cutting edge of a cutting tool coated with the nanolayer of FIG. 1, with a coating of the nanolayer, having a bonding area and an outer area, and also having a finishing layer and a lubricating layer. FIG. It shows the substrate having.

3 is a micrograph of the interface taken via transmission electron microscopy (TEM) technology between the substrate and the coating for the cutting tool coated with the nanolayers of Example 276. FIG.

4 is a micrograph taken of the transmission middle portion via transmission electron microscopy (TEM) technology for the cutting tool coated with the nanolayers of Example 276. FIG.

5 is a micrograph taken through transmission electron microscopy (TEM) of the surface area of the coating for the cutting tool coated with the nanolayers of Example 278.

Referring to the drawings, FIG. 1 shows a particular embodiment of a cutting tool, indicated entirely by reference numeral 20. The cutting tool 20 has an upper inclined surface 22 and a side surface 24. Top inclined surface 22 intersects with side surface 24 to form a cutting edge 26 at the intersection.

As shown in FIG. 2, the cutting tool 20 has a surface 30 with a coating of nanolayers as shown by a bracket, indicated by reference numeral 32. The coating of nanolayers 32 has a bonding area as shown by the brackets indicated by reference numeral 34 in FIG. 2. Bonding region 34 has one or more coatings of nanolayers (and typically has a plurality of coating sets of nanolayers), as described below. The outer region has a plurality of coating sets of nanolayers as described later.

2 shows that a coating of nanolayers 32 has been applied to the side surface (s) 40 and the inclined surface 38 of the substrate 30. However, it should be understood that coating 32 consisting of nanolayers may be applied to selected portions of the surfaces of the substrate, or only to selected ones of the surfaces.

Referring to one arrangement of nanolayer coatings, the nanolayer coating may comprise two or more sets of coatings of alternating layers of materials, where one of the materials is a metal nitride and the other material is a metal aluminum nitride ( For example titanium nitride / titanium aluminum nitride or titanium aluminum nitride / titanium nitride). This means that in one particular coating tissue, the metal nitride (eg titanium nitride) layer may be the layer closest to the surface of the substrate. However, for other specific coating tissues, the metal aluminum nitride (titanium aluminum nitride) layer may be the layer closest to (or actually above) the surface of the substrate. Applicants believe that metal nitrides of the following metals and their alloys, and metal aluminum nitrides, would be acceptable for use in the coating of nanolayers; Titanium, niobium, hafnium, vanadium, tantalum, zirconium, and / or chromium may be provided alone or in combination with each other or in combination with other metals. The metal nitride layer may comprise aluminum as long as the composition of the metal nitride layer is different from that of the metal aluminum nitride layer. Metal nitrides and metal aluminum nitrides may each comprise carbon and / or silicon (as an optional configuration).

Referring to another arrangement of nanolayer coatings, the nanolayer coating may have two or more coating sets of alternating layers of material, where one of the materials is a metal aluminum nitride and the other material is a metal aluminum carbon Nitride (eg titanium aluminum nitride / titanium aluminum carbon nitride or titanium aluminum carbon nitride / titanium aluminum nitride). This means that in one particular embodiment, the metal aluminum nitride (eg, titanium aluminum nitride) layer may be the layer closest to (or substantially over) the surface of the substrate. However, in other particular coating tissues, the metal aluminum carbon nitride (eg titanium aluminum carbon nitride) layer can be the layer closest to (or substantially over) the surface of the substrate. Along the lines of metal nitride / metal aluminum nitride coating sets, Applicants believe that the following metals and their alloys would be acceptable for use with coatings of nanolayers: titanium, niobium, hafnium, vanadium, tantalum, Zirconium, and / or chromium may be used alone or in combination with each other, or in combination with other metals. The metal aluminum nitride may comprise carbon and / or silicon (as optional components). The metal aluminum carbon nitride may comprise silicon (as an optional configuration).

Referring to another arrangement of nanolayer coatings, nanolayer coatings may include alternating layers of metal nitrides, metal aluminum nitrides, and metal aluminum carbon nitrides. Various arrangements of these nanolayers are as follows when the metal is titanium: titanium nitride / titanium aluminum nitride / titanium aluminum carbon nitride or titanium aluminum carbon nitride / titanium aluminum nitride / titanium nitride or titanium aluminum carbon nitride / titanium nitride / titanium Aluminum nitride or titanium aluminum nitride / titanium aluminum carbon nitride / titanium nitride or titanium nitride / titanium aluminum carbon nitride / titanium aluminum nitride or titanium aluminum nitride / titanium nitride / titanium aluminum carbon nitride.

In one group of such arrangements having titanium as the metal, the titanium nitride layer may be the layer closest to (or substantially above) the surface of the substrate. In this group, the titanium aluminum nitride layer and the titanium aluminum carbon nitride layer are different layers.

In another group of such arrangements, the titanium aluminum nitride layer may be the layer closest to (or substantially over) the surface of the substrate. In this group, the titanium nitride layer and the titanium aluminum carbon nitride layer are different layers.

In another group of such arrangements, the titanium aluminum carbon nitride layer may be the layer closest to (or substantially over) the surface of the substrate. In this group, the titanium nitride layer and the titanium aluminum nitride layer are different layers.

Although certain compounds for the coating arrangements described above are titanium nitride, titanium aluminum nitride, and titanium aluminum carbon nitride, metal aluminum nitride and metal aluminum carbon nitride are acceptable. In this regard, metal nitrides, metal aluminum nitrides, and other metals for metal aluminum carbon nitrides, and their alloys, may be niobium, hafnium, vanadium, tantalum, zirconium, and / or chromium alone or in combination with each other, Or in combination with other metals. The metal nitride layer may include aluminum provided that the composition of the metal nitride layer is different from that of the metal aluminum nitride layer and the metal aluminum carbon nitride layer. In the above arrangements, the metal nitride (eg titanium nitride) and the metal aluminum nitride (eg titanium aluminum nitride) may each be provided with carbon and / or silicon (as one option). Metal aluminum carbon nitride (eg titanium aluminum carbon nitride) may be provided with silicon as an optional configuration.

Referring again to the particular coating structure shown in FIG. 2, the junction region 34 includes a plurality of coating sets of alternating nanolayers of titanium nitride and titanium aluminum nitride. The purpose of the bonding area is to provide good adhesion between the coating and the substrate during use (eg, during the application of metal cutting). The junction region has a thickness in the range between about 0.025 micrometers and about 0.6 micrometers. More preferably, the junction region has a thickness that ranges between about 0.05 micrometers and about 0.4 micrometers. Each nanolayer in the junction region has a thickness that can range between about 0.5 nanometers and about 5 nanometers (whether it is a nanolayer of titanium nitride or a nanolayer of titanium aluminum nitride), more preferably, about And may range between 0.5 nanometers and about 2 nanometers.

The thickness of titanium aluminum nitride is typically different from the thickness of the titanium nitride layer. Generally speaking, the thickness of the coating layer changes due to one or more factors, which are set as follows without limitation.

Coating sets having a junction area are deposited during the so-called "ramp up" portion of the coating process. The “lamp up” portion of the process occurs during the initial portion of the process, where the deposition rate of the nanolayer thickness is increased from the first level to the second level. Although it was time consuming to complete the “lamp up” portion of the process, the number of coating sets in the layers was hundreds because each coating set had a thickness in the range of nanometers (ie less than about 100 nanometers thick). Can be increased.

As a result of this continuous increase in deposition rate during the ramp up period, the thickness of the coating sets in the junction area changes. More specifically, as one of the coating sets is located farther from the surface of the substrate, the thickness of each coating set is typically (until the thickness of each coating set reaches a point where the coating sets exhibit a generally consistent thickness). Incremental) is a common case. In the process, the deposition rate increases during the ramp up period, resulting in an increase in thickness. The increase in deposition may be due to one or more of the following factors (without limitation). Gas composition in the chamber, gas flow rate in the chamber, sputtering rate of the target, and / or level of power supplied to the target.

The increase in the thickness of each coating set may be due to the respective nanolayers that are increasing in thickness. Alternatively, an increase in the thickness of each coating set may occur when the thickness of one nanolayer is substantially constant and the thickness of the other nanolayer increases.                 

In the process, for example, once the power to the target has reached a second level of power, the power is preferably at least the first level of power for at least one of the targets so that the rest of the coating process is applied to the outer region. Will be reduced to a greater level. The reduced level of power may be different for each target. In addition, the level of power applied to each target may vary during the portion of the process to apply the outer region.

Referring to the junction region, for example, if the amount of aluminum is less than that contained in the titanium aluminum nitride layers and the titanium aluminum carbon nitride layers, the aluminum content of the titanium nitride layer and the titanium carbon nitride layer in the level range of 0 to higher level. It may be provided.

Referring to FIG. 2, the plurality of coating sets with outer regions are alternating nanolayers of titanium nitride and titanium aluminum nitride. In applications of metal working, the outer region has a thickness in the range of between about 1 micrometer and about 20 micrometers, provided there is good adhesion between the coating and the substrate. More preferably, the outer region has a thickness in the range between about 1 micrometer and about 10 micrometers. Each nanolayer (whether it is titanium nitride or titanium aluminum nitride) has a thickness that can range between about 0.5 nanometers and about 20 nanometers. More preferably, the thickness of each such nanolayer ranges between about 0.5 nanometers and about 10 nanometers. Most preferably, the thickness of each such nanolayer is between about 0.5 nanometers and about 2 nanometers.                 

The thickness of each coating set set in the outer region can be substantially equivalent or can vary. In situations where the coating sets have substantially equal thicknesses, the nanolayers that make up the coating set, ie, the aluminum nitride nanolayer and the titanium aluminum nitride nanolayer, do not necessarily have to be the same. In fact, as can be understood from the following description of the coating tissue shown in FIG. 3, the thickness of the titanium nitride nanolayers ranges from about 1 nanometer to about 2 nanometers and the thickness of the titanium aluminum nitride nanolayers is about Range from 10 nanometers to about 11 nanometers. In this regard, the thickness of the titanium nitride nanolayers in the junction region also ranges between about 1 nanometer and about 2 nanometers, while the thickness of the titanium aluminum nitride nanolayer increases as the coating sets are located farther from the substrate. Applicants believe that the titanium aluminum nitride nanolayer may preferably range in thickness from about 0.5 to about 11 nanometers.

As mentioned above, since the sputtering ratio for a titanium aluminum target is larger than the sputtering ratio for a titanium target, generally speaking, the thickness of each nanolayer of titanium aluminum nitride is greater than that of each nanolayer of titanium nitride. Can be large.

Referring to FIG. 2, layer 50 is a finishing layer that may comprise titanium nitride or titanium aluminum nitride. The thickness of the finishing layer 50 is between about 0.1 micrometers and about 3 micrometers. Applicants believe that metal nitrides, metal aluminum nitrides, and metal aluminum carbon nitrides are acceptable as finish layers. In this regard, other metals and their alloys for metal nitrides, metal aluminum nitrides, and metal aluminum carbon nitrides may comprise titanium, niobium, hafnium, vanadium, tantalum, zirconium, and / or chromium alone or in combination with each other. Or in combination with other metals. As an alternative or in addition to the finishing layer above, the finishing layer may be an alumina layer. Finishing layers are typically applied by physical vapor deposition (PVD) techniques. Layer 52 is a lubricious layer that may include a material such as molybdenum disulfide. The overall thickness of the finishing layer 50 and the lubricating layer 52 is between about 0.1 micrometers and about 3 micrometers. The finishing layer and the lubricating layer are each optional layers for the coating tissue.

Referring to FIG. 2, the substrate 30 is typically a hard material, such as cemented carbide. One exemplary composition for substrate 30 to be substrate A is a cemented (cobalt) tungsten carbide material, which is up to 0.1 weight percent tantalum, up to 0.1 weight percent niobium, up to 0.1 weight percent titanium , From about 0.3 to about 0.5 weight percent of chromium, from about 5.7 weight percent to 6.3 weight percent of cobalt and the remainder of tungsten and carbon, with most of the tungsten and carbide being in the form of tungsten carbide. The substrate has a Rockwell A hardness of about 92.6 to about 93.4, coercive force (Hc) between about 250 to about 320 orersteds, specific gravity of grams per cubic centimeter of about 14.80 to about 15.00, 1-5 Tungsten carbide particle size of micrometer and magnetic saturation of microtesla cubic meter per 167.7 to 191.9 kilogram cobalt. As will be described later, the coated cutting inserts used in the turning test had a substrate of the same composition as the substrate A.

Another exemplary composition for a substrate to be substrate B is a cemented (cobalt) tungsten carbide material, which is about 1.2 to about 2.5 weight percent tantalum, about 0.3 to about 0.6 weight percent niobium, up to 0.4 weight percent Of titanium, having between 11 and 12 weight percent of cobalt and the remainder of tungsten and carbon, with most of the tungsten and carbide being in the form of tungsten carbide. The substrate has a nominal hardness of about 89.8 Rockwell A, a coercive force (Hc) of about 145 to about 185 austeds, a specific gravity of about 14.1 to about 14.5 grams per cubic centimeter, tungsten carbide particle size of 1-6 microns, and 167.7 to 187.9 kilograms have a magnetic saturation of microtesla cubic meters per cobalt. As will be described later herein, the coated cutting insert used in the milling test was provided with a substrate of the same composition as the substrate (B).

The substrate may be a cermet, ceramic or high speed steel, polycrystalline cubic boron nitride, polycrystalline diamond or diamond sheet or diamond film. Substrates are in the form of indexable cutting inserts, cutting inserts, drills, milling cutters, end mills, reamers or taps made from any of the above substrate materials. Can be taken.

The preferred adhesion strength of the coating to the surface of the substrate is at least 45 kilograms (Kg). More specifically, the adhesion strength is at least 60 kg, most preferably the adhesion strength is at least 100 kg. The test to determine adhesion strength is the Rockwell A indentation test.

The preferred thickness of the entire nanolayer coating, excluding the finishing layer and the lubricating layer, is between about 1 micrometer and about 21 micrometers, more preferably between about 1 micrometer and about 21 micrometers, most Preferably the thickness of the coating of the entire nanolayer is between about 2 micrometers and about 6 micrometers.

Generally speaking, the process of making a coating involves using physical vapor deposition, such as electron tube sputtering. In the following examples, the apparatus used to apply the coating was a Semicon CC800 / 8 electron tube sputtering coating reactor. The coating reactor was configured such that the cutting insert substrates were rotated between two sets of targets. Each set of targets was placed 180 ° from the other set. One of the sets of targets was two targets of titanium and the other of the sets of targets was two titanium-aluminum targets. The substrate table was rotated at a rate of 0.8 revolutions per minute. The substrates were mounted on a planetary rod fixture that rotated on a substrate table.

In these examples, the process has two basic parts. The first is the so-called "ramp up" portion, which increases the power to the target from about 500 watts, for example about 8000 watts, over a period of about 45 minutes. Once the power has reached its goal, as an alternative, it is adjusted to remain constant (eg, a power level of 8000 watts or lower) through the rest of the coating process. As another option, the power can be varied during the rest of the coating process. The characteristic of the change can be, for example, a sinusoidal wave, square tooth wave or saw tooth wave.

The following examples are made in a manner that is generally consistent with the above descriptions of the coating process. Each example in Table 1 includes substrates having the same composition as the composition of the substrate A and substrates having the same composition as the composition of the substrate B. The titanium target was a solid titanium metal. The titanium-aluminum target was equipped with a titanium metal target with a plug of 48 aluminum therein. Process parameters for each of these examples are set forth in Table 1 below.

Table I

Process Parameters for Examples of Titanium Nitride / Titanium Aluminum Nitride Nanolayer Coatings

Yes Ti target power (KW) TiAl target power (KW) Argon flow rate (sccm) Nitride flow rate (sccm) Coating time (hours) Bias Current (Amps) Partial flow of nitride 274 4 6 175 -113 6 21 0.31 276 4 8 175 -120 6 26 0.32 277 8 4 175 -119 6 25 0.32 281 4 6 175/100 -180 6 20 0.5 418 1.6 8 210 -90 6 21 0.24 422 1.6 8 210 -88 6 20 0.24

In each of these examples, the flow rate for Krypton was 80 standard cubic centimeters per minute (sccm). In Table I, "sccm", an indication of argon and nitrogen flow rates, is the standard cubic centimeters per minute. In Table I, the partial flow rate of nitrogen is equal to the flow rate of nitrogen (sscm) divided by the sum of the flow rates of nitrogen, argon and krypton (sscm). For Example 281 of Table I, an argon flow rate of 175 sccm was present at the beginning of the ramp up cycle and was reduced to a flow rate equivalent to 100 sccm during the ramp up cycle, which was maintained for the remainder of the coating process.

In processing, there is a control over the aluminum content of titanium aluminum nitride depending on the particular metal cutting application. For some applications, it is generally desirable for the aluminum / titanium atomic ratio (Al / Ti atomic ratio) to be less than 1.0. In this application, the preferred range for the Al / Ti atomic ratio is between about 0.2 and about 0.9. For other applications, it is generally preferred that the Al / Ti atomic ratio is greater than or equal to 1.0, with a preferred range for the Al / Ti atomic ratio being between 1.0 and about 2.5. The limit of the higher end range is based on the ability of the coated cutting insert to have a suitable hardness for metal cutting applications.

To increase the Al / Ti atomic ratio, it is possible to increase the level of power to the aluminum-containing target (s) and / or control the partial flow rate of nitrogen. In order to obtain the maximum aluminum content at a constant power for the aluminum containing target, the partial flow rate of nitrogen can be reduced. The partial flow rate of one preferred nitrogen is less than 0.5. More preferred partial flow rates of nitrogen are less than 0.4. Partial flow rates of more preferred nitrogen are in proportions less than 0.35. If the partial flow rate of nitrogen is less than 0.2, the adhesion and hardness of the layers is reduced. Overall, the preferred range for partial flow of nitrogen is between 0.2 and 0.35.

Table II below describes the process parameters for Example 449. The ramp up for P 449 was the same as in the previous example except that the titanium titanium target was replaced by the titanium-aluminum-carbon target. Each titanium-aluminum-carbon target had twelve plugs of graphite and twelve plugs of aluminum in the titanium metal target.

Table II-Process Parameters for Example 449

(Titanium aluminum carbon nitride / titanium aluminum nitride nanolayer coating)

Yes TiAlC Target Power (KW) TiAl target power (KW) Argon flow rate (sccm) Nitrogen Flow Rate (sccm) Coating time (hours) Bias Current (Amps) Nitrogen fractionation ratio 449 8 1.6 210 87 6 15 0.23

For the treatment of Example 449, the flow of krypton gas was kept constant at a rate of 80 standard cubic centimeters per minute. In Table II, the indication of “sccm” for argon and nitrogen flow rates is standard cubic centimeter per minute.

Table III below is the process variables for Example 394. The ramp up for Example 394 was the same as Example 449 except that the titanium-aluminum target was replaced by the titanium target. Each titanium-aluminum-carbon target had 12 plugs of aluminum and 12 plugs of graphite in the titanium metal target.

Table III-Process Parameters for Example 394

(Titanium aluminum carbon nitride / titanium nitride nanolayer coating)

Yes TiAlC Target Power (KW) Ti target power (KW) Argon flow rate (sccm) Nitrogen Flow Rate (sccm) Coating time (hours) Bias Current (Amps) Nitrogen fractionation ratio 394 8 1.6 210 80 6 20 0.22

For the treatment of Example 394, the flow of krypton gas was kept constant at a rate of 80 milliliters per minute. In Table III, the indication of "sccm" for argon and nitrogen flow rates is standard cubic centimeters per minute.

Selected properties of the resulting coated cutting tool are shown in Table IV below. These properties include the microhardness of the cutting tool in kilograms per square millimeter (kg / mm ² ) measured by the standard Vickers test at an aluminum / titanium atomic ratio, the overall thickness of the coating in micrometers, and a load of 25 grams. (microhardness), indent adhesion strengths of coated cutting tools measured in kilograms.

Referring to the analysis of the coating layers, a JEOL 6400 Scanning Electron Microscope (SEM) with an INCA Energy 400 Dispersive X Ray Spectrometer (EDS) from Oxford Industries was used to coat the coating (ie, titanium aluminum nitride coating). Collect composition information regarding Oxford Industries is located at 130A, Baker Avenue Ex, Concord, MA 01742. JEOL USA, Inc. is located at 11, Dearborn, Peabody, MA 01960.

The coating is analyzed either in preparation of additional samples or in a deposited state without a conductive coating applied. X-rays are focused using an acceleration voltage of 15 KV.

The coating should be at least about 3 micrometers thick to prevent excitation of the substrate by the electron beam (a thicker coating would be required if higher acceleration voltages were used). At least five spectra were collected and the results quantified. The apparent concentration of each element is equal to the intensity of the element in the sample multiplied by the weight percentage of the standard element divided by the intensity of the standard element. This should be corrected for the effect between the elements such that the weight percentage of the elements is equal to the apparent concentration divided by the strength correction. The atomic percentage is then calculated by dividing the weight percentage by the atomic weight of the urea. There are several ways to calculate the intensity correction. This particular analysis instrument uses a Phi-Rho-Z approach. Since the correction factors depend on the composition of the sample, the actual concentrations are derived using iterative calculations.

Table IV

Selected Characteristics of Examples Using Substrate A

Yes Al / Ti atomic ratio (%) Thickness (μm) Average value of Vickers micro hardness (Kg / mm ² ) Indentation adhesive strength (kg) 274 0.6 3.4 / 4.1 / 3.4 2770 ± 101 > 60 276 0.67 3.9 / 4.1 / 3.8 3051 ± 133 > 60 277 0.25 4.1 / 3.9 / 3.6 2856 ± 071 > 60 281 0.46 3.2 / 2.8 / 2.9 2767 ± 169 > 60 418 1.1 4.5 / 5.6 / 5.3 2774 ± 32 > 60 422 1.18 3.6 / 3.6 / 4.0 2818 ± 245 > 60 394 0.24 [4.9 atomic% carbon present] 4.2 / 4.1 / 4.0 3016 ± 133 > 60 449 0.36 [with 2.9 atomic% carbon] 4.4 / 4.2 / 3.9 2899 ± 60 > 60

The examples shown in Table IV used substrates that had the same composition as that of substrate A. For the properties listed in Table IV, Applicants expect that coated cutting inserts using a substrate that had the same composition as substrate B would exhibit the same or substantially similar properties.

Some examples have been tested in applications of turning. The parameters for turning are: working material is 304 stainless steel, speed is 500 surface feet per minute (sfm) [152 meters per minute], feed is 0.012 inches per revolution (ipr) (0.3 per revolution) Millimeters), the depth of cut is 0.080 inches (doc) (2 millimeters doc) and a float coolant was used. The cutting tool was CNGP432 of the cutting tool with a negative five degree lead angle and a sharp cutting edge. The results of the turning test are shown in Table III below.

The criterion for tool life is as follows: uniform flank wear: 0.012 inches (0.3 millimeters); Maximum flank wear: 0.015 inches (0.4 millimeters); Nose wear: 0.016 inches (0.4 millimeters); Crater wear: 0.004 inches (0.100 millimeters); Chip width on rake: 0.020 inch (0.5 millimeter); Depth of cutting notch: 0.016 inch (0.4 mm).

Table V

Tool life (minutes) for 304 stainless steel

Yes Rep. One Rep. 2  Average  Std. Deviation 277 18.00 14.30 16.15 2.62 274 14.93 23.56 19.24 6.11 281 12.46 11.00 11.73 1.03 276 27.28 21.66 24.57 3.97 KC5010 [Comparative Example] 14.00 16.00 15.00 1.41

For Comparative Example KC5010, the substrate had the same composition as the substrate (A). The coating was a single layer of titanium aluminum nitride with a nominal thickness of about 4.0 micrometers. Referring to Comparative Example KC 5010, the Al / Ti ratio was approximately equal to 1.0, and the microhardness was equal to about 2500 Kg / mm ² . KC 5010 cutting tools are manufactured by Kennametal Inc. of Latrobe, PA. Prior art cutting tools available from.

Referring to FIG. 3, the outer area and the bonding area of the coated tissue from Example 276 are shown. For each one of the junction region and the outer region, there are alternating nanolayers of titanium nitride and titanium aluminum nitride. Dark nanolayers are titanium nitride and light nitrides are titanium aluminum nitride.                 

With respect to FIGS. 3 and also 4 and 5, Applicants believe that visual contrast in the dark areas between the nanolayers indicates that the titanium nitride nanolayer does not have aluminum contained therein, or titanium It should be understood that significantly less aluminum is contained therein than the aluminum nitride nanolayer has. It is to be understood that the titanium nitride nanolayers may comprise aluminum and therefore need not necessarily be pure titanium nitride. To the extent that aluminum is included in the titanium nitride nanolayers, this aluminum content can vary between the titanium nitride nanolayers. Applicants believe that the dark spots in the figures, and in particular in FIG. 3, are the product of TEM sample preparation.

Referring to the junction region, the nanolayers of titanium nitride have a thickness between about 1 and 2 nanometers. The thickness of the titanium nitride nanolayers remains substantially constant throughout the junction region. The thickness of the titanium aluminum nitride nanolayers begins at a range between about 1 and about 2 nanometers at and near the interface between the coating and the substrate. The substrate is a black area in the upper right corner of the micrograph. The thickness of the titanium aluminum nitride layers increases as one of them is located farther from the surface of the substrate. The thickness of the titanium aluminum nitride nanolayers increases in the range between about 10 and about 11 nanometers.

Referring to the micrograph of FIG. 4, a bulk region of the coated tissue is shown. The bulk region has alternating nanolayers of titanium nitride and titanium aluminum nitride with one nanolayer of titanium nitride and one nanolayer of titanium aluminum nitride having a coating set. The thickness of each nanolayer of titanium nitride is about the same and ranges from about 1 to about 2 nanometers. Each nanolayer thickness of titanium aluminum nitride is about the same and ranges between about 10 nanometers and about 11 nanometers.

Referring to the micrograph of FIG. 5, an area of coated tissue having an outer surface is shown. This area of the coating tissue has alternating nanolayers of titanium nitride and titanium aluminum nitride, with one nanolayer of titanium nitride and one nanolayer of titanium aluminum nitride having a coating set. The thickness of each nanolayer of titanium nitride is about the same and ranges from about 1 to about 2 nanometers. The thickness of each nanolayer of titanium aluminum nitride is about the same and ranges between about 10 nanometers and about 11 nanometers.

Examples have been tested in the application of milling. The milling parameters are as follows: the working material is 4140 steel, the speed is 600 surface feet per minute (sfm) [183 meters per minute], the feed is 0.012 inches per revolution (ipr) [0.3 millimeters per revolution], The axial depth (adoc) of the cut was 0.100 inch [2.5 millimeters rdoc], the radial depth (rdoc) of the cut was 3.0 inches [75 millimeters rdoc], and full coolant was used. The cutting tool was a SEHW43A6T type of cutting tool with a lead angle of 45 degrees and a T mill of 0.2 millimeters and 20 degrees. The results of the milling test are shown in Table VI below.

The criterion for tool life was as follows: uniform flank wear: 0.012 inches (0.3 millimeters); maximum flank wear: 0.016 inches (0.4 millimeters); Nose wear: 0.016 inches (0.4 millimeters); Crater wear: 0.004 inches (0.100 millimeters); Chip width on rake: 0.030 inch (0.75 millimeters). The examples shown in Table VI used a substrate that had the same composition as the substrate (B). Comparative example KC525M is a cutting tool with a substrate having the same composition as the composition of substrate B and a coating of titanium aluminum nitride, the coating having a nominal thickness of about 4 micrometers.

Table VI

Tool life (minutes) for milling 4140 steel

Yes Rep.1 Rep.2 Rep.3 Average tool life / Std. Deviation 277 7.45 6.62 9.10 7.72 / 1.26 274 7.45 8.28 8.28 8.00 / 0.48 281 4.96 7.45 8.28 6.90 / 1.73 276 8.28 4.97 8.28 7.18 / 1.91 KC525M [Comparative Example] 4.97 4.97 6.62 5.52 / 0.96

Patents identified herein and other documents are incorporated herein by reference.

Other embodiments of the invention will be apparent to those skilled in the art from consideration of the practice and detailed description of the invention disclosed herein. The specification and examples are exemplary only and are not intended to limit the scope of the invention. The true scope and spirit of the invention is defined by the following claims.

The present invention can be applied to cutting tools and the like.

Claims (128)

A substrate having a surface and a coating on the surface of the substrate; The coating has a plurality of coating sets of nanolayers, each coating set having alternating nanolayers of metal nitride and metal aluminum nitride; The coating has a bonding area and an outer area; And, The bonding area has a plurality of coating sets, the thickness of the coating sets increasing as one of the coating thicknesses is located away from the surface of the substrate. delete delete delete delete delete The method of claim 1, Wherein each one of the metal aluminum nitride nanolayers and each one of the metal nitride nanolayers in the junction region has a thickness between 0.5 nanometers and 5 nanometers. The method of claim 1, Wherein each one of the metal aluminum nitride nanolayers and each one of the metal nitride nanolayers in the junction region has a thickness between 0.5 nanometers and 2 nanometers. delete The method of claim 1, Wherein each one of the metal aluminum nitride nanolayers in the outer region and each one of the metal nitride nanolayers have a thickness between 0.5 nanometers and 20 nanometers. delete delete The method of claim 1, The metal is titanium, for each coating set the titanium aluminum nitride nanolayer has a thickness and the titanium nitride nanolayer has a thickness, wherein the thickness of the titanium aluminum nitride nanolayer is different from the thickness of the titanium nitride nanolayer. Coated member of the nanolayers. The method of claim 1, The metal is titanium, for each coating set the titanium aluminum nitride nanolayer has a thickness and the titanium nitride nanolayer has a thickness, wherein the thickness of the titanium aluminum nitride nanolayer is greater than the thickness of the titanium nitride nanolayer. Coated member of the nanolayers. delete delete The method of claim 13, Each nanolayer of titanium aluminum nitride in the junction region has a thickness in the range of between 0.5 nanometers and 11 nanometers. delete delete delete delete delete delete delete The method of claim 1, The coated member of the nanolayers comprises: a nanolayer comprising one of a cutting insert, an indexable cutting insert, a drill, a milling cutter, an end mill, a reamer and a tap Coated member. delete The method of claim 1, And a finishing layer applied to the outer surface of the coating. delete delete The method of claim 1, The coated member of the nanolayer, wherein the ratio of aluminum / titanium atoms in the metal aluminum nitride nanolayer is in the range of 0.2 to 2.5. delete The method of claim 1, The coated member of the nanolayer, wherein the aluminum / titanium atomic ratio is greater than 0.2 and less than 0.9. The method of claim 30, And the aluminum / titanium atomic ratio is greater than or equal to 1.0 and less than 2.5. delete delete delete delete delete delete delete delete delete delete delete delete delete delete delete delete delete delete delete delete delete delete delete delete delete delete delete delete delete delete delete delete delete delete delete Providing a substrate having a surface; Providing a metal target; Providing a metal aluminum target; Rotating the substrate between the metal target and the metal aluminum target; Supplying power to the metal target at a first level; Supplying power to the metal aluminum target at a first level; Depositing a coating having alternating coating sets of nanolayers on the surface of the substrate; Varying the deposition rate of alternating nanolayer thickness over a first time period in which the power supplied to the metal target and the metal aluminum target is changed from the first level to the second level; And, Controlling the deposition rate of alternating nanolayer thicknesses during the second time period after the power reaches the second level. The method of claim 69, And wherein said alternating nanolayers comprise metal nitrides and metal aluminum nitrides. The method of claim 69, The alternating nanolayers comprise a metal nitride and a metal aluminum nitride, and the depositing step is a time at which power for the metal target and the metal aluminum target changes from the first level to the second level to deposit the junction region of the coating. While depositing a plurality of coating sets of said alternating nanolayers. The method of claim 71 wherein Each coating set provided in the bonding area has a thickness, and the thickness of the coating sets in the bonding area increases as one of the coating sets is located away from the surface of the substrate. Way. delete delete delete delete delete delete delete The method of claim 69, The coated layer of nanolayer comprises one of a cutting insert, an indexable cutting insert, a drill, a milling cutter, an end mill, a reamer, and a tap. A method of making a coated member. The method of claim 69, After providing the metal aluminum target, supplying nitrogen at a preselected partial flow rate. 82. The method of claim 81 wherein Wherein the nitrogen fractionation ratio is 0.5 or less. 82. The method of claim 81 wherein The nitrogen fractionation ratio is 0.4 or less. 82. The method of claim 81 wherein The nitrogen fractionation ratio is in the range of 0.35 to 0.2. The method of claim 69, Wherein the first level of power is less than the second level of power. delete delete delete delete delete delete delete delete delete delete delete delete delete delete delete delete delete delete delete delete delete delete delete delete delete delete delete delete delete delete delete delete delete delete delete delete delete delete delete delete delete delete delete

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